1,8-Diazabicyclo(5.4.0)undec-7-ene → N-ethyl-N'-[7-(phenylsulfanyl)-4,5-dihydro-1,3-benzothiazol-2-yl]urea

HRID 9159ノート

反応式

HRID 9159 の反応式
[C:1]1([S:7][C:8]2(SC3C=CC=CC=3)[C:16]3[S:15][C:14]([NH:17][C:18]([NH:20][CH2:21][CH3:22])=[O:19])=[N:13][C:12]=3[CH2:11][CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1CCN2C(=NCCC2)CC1>C1COCC1>[CH2:21]([NH:20][C:18]([NH:17][C:14]1[S:15][C:16]2[C:8]([S:7][C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)=[CH:9][CH2:10][CH2:11][C:12]=2[N:13]=1)=[O:19])[CH3:22]

参加物

4

反応物 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 21985555N-[7,7-Di(phenylsulfanyl)-4,5,6,7-tetrahydro-1,3-benzothiazol-2-yl]-N'-ethylurea

生成物 1

HCID 21985581N-ethyl-N'-[7-(phenylsulfanyl)-4,5-dihydro-1,3-benzothiazol-2-yl]urea

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

To a suspension of N-[7,7-di(phenylsulfanyl)-4,5,6,7-tetrahydro-1,3-benzothiazol-2-yl]-N′-ethylurea (700 mg, 1.59 mmol) in THF (14.0 mL) was added DBU (0.36 mL, 2.38 mmol). The reaction mixture was stirred at about 20° C. for about 30 min. The reaction was concentrated in vacuo. The residual yellow oil was taken up in CH2Cl2, washed with AcOH/H2O 1/10 and dried over MgSO4. The organic solvent was removed in vacuo and the residual oil (1.0 g) was used in the next step without further purification.

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. washwashed with AcOH/H2O 1/10
  3. dry with materialdried over MgSO4
  4. customThe organic solvent was removed in vacuo
  5. customthe residual oil (1.0 g) was used in the next step without further purification

出典と根拠

ORDレコード
ord-f52c1f5594b74389a752e81d2ba57891
出典データセット
uspto-grants-2006_08
特許番号
US07091227B2

反応ノート

読み込み中…